Micronized calcium carbonate to enhance water-based drilling fluid properties

Advanced drilling technique requires competent drilling fluids. This study tests micronized calcium carbonate (CaCO3) as a water-based drilling fluid (WBDF) additive. CaCO3 microparticles were extracted from Aruma formation outcrop and studied for structural, colloidal stability, morphology, and particle size distribution. WBDF systems were prepared with varying quantities of CaCO3 microparticles, including 0, 15, 30, and 45 lb/bbl, respectively. The addition of CaCO3 microparticles was investigated in terms of the rheological, high pressure-high temperature (HPHT) filtration, barite sagging, density, and pH. The results showed that CaCO3 microparticles are stable at a pH greater than 8. Moreover, fluid containing CaCO3 microparticles exhibited an enhancement in rheological properties. The yield point increased by 29%, 34%, and 37% for 15, 30, and 45 lb/bbl of CaCO3 respectively. In addition, the HPHT filtration also showed that CaCO3 has a significant improvement in both filtration loss and filter cake thickness. The filter cake thickness decreased by 17%, 40%, and 65% at 15, 30, and 45 lb/bbl of CaCO3 respectively. Static and dynamic sag maintained in a safe range at 30 lb/bbl of CaCO3 microparticles. This study showed that using CaCO3 microparticles along with conventional fluid additives improved the thermal stability and rheological properties of drilling fluid.

filtration characteristics of WBMs 21 , shale stability to reinforce the well 22 , hydration and clay swelling 23 , and fluid stability under hard conditions high-pressure high-temperature 24 .
To prevent formation damage from polymers and particles migrating into porous formations, the correct particle size distribution (PSD) of the drilling fluid must be used.When the particle size of CaCO 3 is the same as the pore throat, the formation can be damaged.Particles less than 53 µm invaded ceramic discs with a mean pore-throat size of 50 µm, reducing permeability by 17-18% 38 .Adding cellulose fibers prevented solids and polymers from migrating into the formation.However, many researchers confirm particle diameter should be equal to one-third of the formation pore throat 17 .Small, abundant, low-cost, and safe CaCO 3 particles are attractive drilling fluid additives.CaCO 3 nanoparticles are a modern drilling fluid addition.Bentonite water-based drilling fluids were tested and contained 0.025-0.5% CaCO 3 nanoparticles 39 .CaCO 3 nanoparticles were shown to have a notable effect on filtering characteristics and to produce flatter cake surfaces.To mitigate drilling fluid absorption into the shale matrix, Zhang et al. 40 worked on drilling fluid using CaCO 3 nanoparticles.Maximum permeability decreases in shale matrices of 95.5% were achieved at a nanoparticle concentration of 1%, demonstrating a successful sealing effect.Despite the findings, there are several variables associated with the rheological and viscoelastic properties of fluids with different quantities of CaCO 3 , as well as the barite settling in the drilling fluid.Moreover, optimizing high-pressure high-temperature filtration properties between the various components of WBM, still need to be clarified.
The objective of this research is to establish the optimal concentration of CaCO 3 microparticles for use in a water-based drilling fluid to achieve the desired effects of rheological modification, filtration loss control, and barite settling prevention.Extraction of CaCO 3 from Aruma Saudi formation limestone is followed by milling and sieving as part of the study.Additionally, PSD, SEM, XRD, XRF, and zeta potential are used to characterize the CaCO 3 ; and the effects of various CaCO 3 microparticles vary from 0, 15, 30, and 45 lb/bbl on the most important functional characteristics of WBMs are assessed.

Prepared CaCO 3 particles
Calcium carbonate particles were prepared from limestone rocks in Fig. 1 extracted from Khanasir limestone members of the Aruma Saudi formation.The Khanasir limestone, the Hajajah limestone, and the Lina Shale make up the three main members of this formation, listed from bottom to top.Aruma outcrop in Saudi Arabia has been found in Al-Kharj City southeast of Riyadh in central Saudi Arabia 41,42 .The limestone rock was crushed to fine particles using a ball milling machine.Then sieved to have very fine particles of less than 10 µm.

Characterization of CaCO 3 particles
The particle size distribution (PSD) was analyzed using HELOS particle size analyzer to determine the size distribution of API barite, conventional CaCO 3 (50 µm), and sieved CaCO 3 .The results showed sieved CaCO 3 has a size distribution within a narrow window of distribution.On the other hand, both barite and CaCO 3 (50 µm) have a wide range of particles as shown in Fig. 2. Barite particles and CaCO 3 (50 µm) have a D 50 value of 18 and 34 µm respectively, while sieved CaCO 3 had a value of 2.8 µm.D 50 means 50% of the particles by mass have diameters less than this value.As can be seen in Fig. 2, Sieved calcite has a narrow window of the particle size distribution of very fine particles.
Scanning electron microscopy (SEM) in Fig. 3 showed that micronized CaCO 3 particles had rhombohedral to sub-rounded regular shapes and were similar in size, while barite and conventional CaCO 3 particles were

Drilling fluid preparation
Following the steps in Table 2, the reference water-based drilling fluid named "Base" was prepared by mixing the drilling fluid additives.The water used as the first base fluid was treated with soda ash to keep its hardness consistent.The pH was adjusted with potassium hydroxide, and foam production was suppressed with a defoamer.The mud viscosity was maintained using bentonite and xanthan gum polymer.Then, starch and low viscosity polyanionic cellulose (PAC-LV), and calcium carbonate were employed to enhance the filtration control capability of the drilling fluid.The clay was stabilized with potassium chloride, and the mud's density was increased using barite.At room temperature, a three-speed mixer was used to combine all of the ingredients.To investigate the impact of CaCO 3 particles on the primary functional features of WBMs, several tests were carried out such as pH, density, rheological, HPHT filtration, and sagging properties.

Zeta potential
The test examined the impact of CaCO 3 microparticles on fluid stability by measuring zeta potential at different pH levels.Fluid instability is indicated when the zeta potential falls within 0 to ± 30 mV 43 .Various pH fluid samples were prepared, and pH levels were controlled using KOH and HCl.Then, shaken for 24 h to achieve charge equilibrium.The Zeta potential of CaCO 3 microparticles (0.5 wt%) was measured using Malvern Zetasizer at 75 °F and atmospheric pressure.The value of zeta potential was determined from 3 measurements for each reading of 10 runs.

Rheological and filtration properties
WBM prepared with bentonite, polymers, and various CaCO 3 microparticle concentrations were analyzed for their rheological characteristics.The rheological properties of WBM were evaluated using Fann M3600 viscometer after the drilling fluid hot rolled at 250 °F for 16 h to simulate downhole conditions.The following equations 44 of the Bingham plastic fluid model described are utilized to identify the apparent viscosity (AV), plastic viscosity (PV), and yield point (YP).The gel strength and yield point are stated in lb f /100 ft 2 , and the viscosity is given in centipoise.
(1) AV = RPM 600 2 (2) PV = RPM 600 − RPM 300 The filtration properties at high-pressure high-temperature (HPHT) are performed using Fann HPHT 175 cm 3 filter press.It is advised by API regulations that the HPHT filtrate volume be twice for comparison purposes because the filter press area is half of the regular filter press equipment used for API circumstances.The test was done at a pressure difference of 300 psi and a temperature of 250 °F.As a filtering medium, a filter paper with a mean pore diameter of 2-5 µm was used.The test was done for the usual amount of time, 30 min.The properties of filtration that are measured are the thickness and weight of the filter cake as well as the total filtration volume.

Static and dynamic sag
The ability of a drilling fluid to suspend weighted material at a given temperature and duration is generally measured using static sag.Measurement of the sag factor (SF) was used to assess the mud's sag performance.The sag factor at 250 °F and 500 psi for 24 h was calculated in Eq. ( 4): where ρ bottom and ρ top are the density of drilling fluid from the bottom and top part of the aging cell respectively.Having a sag factor greater than 0.53 indicates that drilling fluid has the potential to settle weighting material below mud 45 .The 6-speed rotational viscometer and thermocouple, standard equipment for measuring mud's rheological properties, served as the inspiration for the viscometer sag shoe test (VSST) design.The thermocouple acts as the mud container and heats the mud to 180 °F (although the test is typically done at 120 °F).While the sag shoe has a sloped surface that directs the weighted material into a single collection well.The viscometer provides a consistent shear (100 RPM) to imitate dynamic circumstances.VSST can be calculated by Eq. ( 5): where w 1 and w 2 are the mass of 10 cm 3 of drilling fluid from the sag show wall at time zero and 30 min respectively.It would be suggested that a drilling fluid with VSST 1.0 lb/gal or less, indicates the least amount of sagging tendency 46 .

Density and pH
The specific gravity of CaCO 3 is 2.75, so adding the different amounts in the high-density drilling fluid will not increase the weight of the drilling fluid.The results in Fig. 5 showed there are no significant changes in the mud density after adding CaCO 3 .The increase in the mud density is only 2.17% after adding 45 lb/bbl.Results from a pH meter reading on the prepared sample are displayed in Fig. 5.The mud without fine CaCO 3 read a pH of 12 and mud with 45 lb/bbl CaCO 3 indicated the same pH value.Both have the same pH value, indicating that the CaCO 3 didn't affect the pH.The reason behind this is due to water-based drilling fluids usually have their pH stabilizer such as KOH, which possesses significantly higher buffering capabilities than calcium carbonate.Furthermore, calcium carbonate is relatively insoluble, and when introduced into water-based drilling fluids, it doesn't fully dissolve.These insoluble calcium carbonate particles exhibit a neutral pH, thereby making no significant contribution to the fluid's pH.

Zeta potential of CaCO 3 microparticles
The zeta potential is a measure of the electric field and can be used to predict the stability of the colloidal system.For example, a high zeta potential (either positive or negative) indicates a strong electric field and a stable www.nature.com/scientificreports/colloidal system, while a low zeta potential indicates a weak electric field and an unstable system.As a result, shown in Fig. 6, CaCO 3 microparticles are stable at a pH greater than 8.This indicated that CaCO 3 microparticles are stable in WBM at conventional pH (i.e.9-12).

Rheological properties
The correlation between the observed shearing rate and the shear stress is depicted in Fig. 7 of non-Newtonian drilling fluids.The graphs show that as the quantity of CaCO 3 is increased in each of the three water-based drilling fluid samples, the shear stress increases within a narrow window.In general, the yield point of 52 lb/100 ft 2 of 45 lb/bbl CaCO 3 can be located where the Bingham plastic fluid line intersects the vertical axis of Fig. 7.
When fluid samples are treated with fine particles of CaCO 3 , the shear stress is higher than for the barite sample.However, at the same concentration of CaCO 3 , shear stress of micronized CaCO 3 is less than 50-micron CaCO 3 .This is attributed to the friction of large particles is higher.Moreover, larger particles tend to settle more quickly while shearing, potentially resulting to a more concentrated layer at the bottom of the viscometer cell.Increased viscosity and shear stress may result from such a high concentration of particles.A Bingham yield point shown in Fig. 8 increased by 29%, 34%, and 37% for 15, 30, and 45 lb/bbl of CaCO 3 respectively.Moreover, 30 lb/bbl of 50-micron CaCO 3 increased the YP to 66%.  as it helps to improve the rate of penetration and enhances hole cleaning 48 .On the other hand, extremely high yield points can induce uncontrolled increases in circulation pressure loss, resulting in significant equivalent circulation density (ECD).High ECD could induce formation damage or high circulation pressures that exceed drilling pump rating.The correlation between gel strength and CaCO 3 concentration at 10 s,10 min, and 30 min is depicted in Fig. 9.The shearing force required to break the gel in drilling fluid is a measure of the fluid's gel strength.As calcium carbonate increased, the gel strength of WBM increased.The gel strength behavior of mud samples after thermal aging testing is shown in Fig. 9.All the CaCO 3 concentrations caused an increase of 30/10 min gels as 32%, 30%, and 24% of 0, 15, and 45 lb/bbl CaCO 3 respectively.However, in the 30 lb/bbl of CaCO 3 , the 30/10 min gelling showed an increase of 6%.This means that adding 30 lb/bbl of CaCO 3 enhances the gel strength of WBM with flat rheology.On the other hand, 30 lb/bbl of 50-micron CaCO 3 increased the 30/10 min gelling by 25%.This increase in gel strength is attributed to dense packing of barite and 50-micron CaCO3 is higher than barite and micronized CaCO3 which leads to higher viscosity.

HPHT filtration properties
Additional mud characteristics studied include high-pressure high-temperature filtrate loss (HPHT FL) and filter cake thickness (HPHT FCT).Both characteristics are depicted in Figs. 10 and 11.An effective drilling mud will prevent formation fracture and formation instability by limiting the amount of filtrate lost to the formation.From what can be shown in Fig. 10, it appears that adding CaCO 3 can significantly improve the base mud filtering control property when its concentration is raised.Increasing the CaCO 3 concentration of 15, 30, 45, and 30 (50 µm) lb/bbl increased HPHT FL control of the base mud by 4.85%, 53.4%, 88.3%, and 47.6%, respectively.Furthermore, the addition of 30 lb/bbl of 50-micron CaCO 3 exhibited filtration control comparable to that of micronized CaCO 3 .This indicates that calcium carbonate can serve as a bridging agent, albeit with some concerns regarding its impact on rheology and stability.
For this reason, it can be concluded that, under the current conditions, 30 and 45 lb/bbl of examined CaCO 3 concentrations are suitable for controlling filtrate loss and avoiding formation fracture and drilling fluid loss.Further analysis of the rheological, sagging, and filtration data collected in this study suggests that 30 lb/bbl of micronized CaCO 3 particles had exceptional properties and a significant degree of temperature stability of water-based drilling fluid.This has a lot of potential in down-hole settings if these features hold up at even higher temperatures.

Static and dynamic sag test
The barite separation in each sample was analyzed by conducting a static sag performance test at 0° and 45° of the base WBM and with calcium carbonate of varying concentrations.Drilling fluids' sag factors after 24 h of static aging are shown in Fig. 12.In comparison to employing barite as a weighing material, the results showed that blinding barite with micronized calcium carbonate decreased the possibility of solids separation and sag factor occurrence.After including 30 lb/bbl of micronized CaCO 3 , the sag factor of the WBM was brought down to the safe range for both vertical and inclined configurations.Because 30 lb/bbl of 50-micron CaCO 3 has a higher yield point and gel strength, it prevents the static settling of barite.This is because when the fluid is at rest, the gel strength builds up, keeping the solids in suspension.
The extent of the dynamic sag was quantified using the value of the VSST.Drilling fluid with a VSST of 1 ppg or less has a low sagging tendency, whereas a VSST greater than 1 ppg suggests the possibility of a sagging issue.The results in Fig. 13 indicated that adding CaCO 3 to the drilling fluid enhanced the settling of barite particles.Similar to static sag, CaCO 3 of 30 and 45 lb/bbl prevented the barite from settling in the drilling fluid.The reason behind these as small particles of CaCO 3 of the high surface area increased as shown in Fig. 14, and the free space between the particles decreased.Thus, micronized calcium carbonate is distributed around the barite particles prevents them from settling down.The presence of 30 lb/bbl of 50-micron CaCO 3 were unable to prevent the settling of barite in dynamic conditions.This can be attributed to the larger size of the calcium carbonate particles, which failed to occupy the gaps between the barite particles, even when the drilling fluid had   www.nature.com/scientificreports/ a high viscosity.On the other hand, micronized calcium carbonate with a high surface area effectively reduced the available space between the barite particles, preventing their settling.It is important to note that the particle size distribution plays a crucial role in influencing the sagging stability, which, in turn, affects both rheological properties and sagging stability.In summary, achieving an appropriate particle size distribution for total solids is of paramount importance in influencing both rheological properties and sagging stability.

Conclusions
Micronized calcium carbonate was used in this work with different concentrations (0, 15, 30, and 45 lb/bbl) to improve the viscosity, filtration, and stability of the barite drilling fluid.The effect of these concentrations on the drilling fluid properties was investigated with the following conclusions: • The CaCO 3 microparticles are stable in alkaline drilling fluids.Zeta potential maintained to the stable range after pH greater than 8. • The rheological properties showed that CaCO 3 microparticles can be used at (250 °F).The YP raised by 29%, 34%, and 37% for 15, 30, and 45 lb/bbl of CaCO 3 microparticles.As well as the gel strength increased with CaCO 3 microparticles.• CaCO 3 microparticles enhanced the filtration control capability by decreasing the filtrated volume from 20.6 to 19.6, 9.6, and 2.4 cm 3 and decreasing the filter cake thickness by 17%, 40%, and 65% for 15, 30, and 45 lb/ bbl of CaCO 3 microparticles respectively.• Under both static and dynamic circumstances, the sag factors were maintained at safe levels when 30 lb/bbl of CaCO 3 was added to the barite drilling fluid.• The overall properties of the drilling fluid showed that 30 lb/bbl of CaCO 3 microparticles was enough to enhance all its functions at both normal and 250 °F.

Figure 7 .
Figure 7.The shear rate vs. shear stress and apparent viscosity of WBM after hot rolling 250 °F.

Figure 9 .
Figure 9.The gel strength of WBM after hot rolling 250 °F.
47.5, and 57.45° which is similar to conventional CaCO 3 .The X-ray fluorescence was used by M4 TORNADO PLUS to determine the elemental composition of conventional and micronized CaCO 3 .The results are shown in Table1.Micronized CaCO 3 has Ca more than conventional and CaCO 3 .